CN112608720B - High-thermal-conductivity interface material and preparation method thereof - Google Patents
High-thermal-conductivity interface material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of interface materials, in particular to a high-thermal-conductivity interface material and a preparation method thereof. The invention mainly develops a heat-conducting gel material which has ultrahigh heat conductivity coefficient and is used for an automatic dispensing process. The heat-conducting gel comprises the following components: 3-4 kinds of high heat-conducting powder fillers with different particle size ranges and one or two kinds of matched silane coupling agents. Through the collocation and the processing of filler for the addition of filler increases, thereby accomplishes the purpose that promotes coefficient of heat conductivity, for the constantly growing application of heat dissipation capacity provides the heat dissipation scheme, for the chip protection driving that calorific capacity constantly increases. Specifically, the first aspect of the present invention provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the content of the micron-sized inorganic filler is at least not lower than 55 wt% of the high-thermal-conductivity interface material, so that the thermal conductivity coefficient of the interface material reaches 8-10W/m-K, and the micron-sized inorganic filler has excellent rheological property and can meet the requirement of an automatic dispensing process.
Description
Technical Field
The invention relates to the technical field of interface materials, in particular to a high-thermal-conductivity interface material and a preparation method thereof.
Background
With the increasing integration of electronic components, the requirements for processing and operating speed, storage density, energy density, etc. are also increasing, and high temperature will have harmful effects on the stability, reliability and life of the electronic components. Thermally conductive interface materials play a crucial role in the thermal management of electronic devices. Meanwhile, under the promotion of the rapid development in the fields of 5G, new energy and the like, the demand for more efficient and stable heat-conducting interface materials is rapidly increased.
Generally, the thermal conductivity of the heat conductive material is in direct proportion to the addition amount of the filler. On one hand, the filler cannot be added up after being added to a certain amount, otherwise the filler cannot be well formed and influences normal use, the limit of the thermal conductivity of the filler can only be about 5W/m-K, and the requirement of a high-performance electronic device cannot be effectively met. On the other hand, most of the heat conducting interface materials on the market are made of silicone rubber crosslinked by vinyl silicone oil, and because the filler content is low and the silicone rubber content is high, a large amount of uncrosslinked silicone oil exists in the heat conducting interface materials, and the uncrosslinked silicone oil can slowly seep out under the action of pressure in the actual use process of the silicone oil, so that electronic components are polluted, and particularly, the heat conducting interface materials have fatal influence on the components under the environment sensitive to the silicone oil.
Disclosure of Invention
Aiming at the technical problems, the invention mainly develops a heat-conducting gel material which has ultrahigh heat conductivity coefficient and is used for an automatic dispensing process. The heat-conducting gel comprises the following components: 3-4 kinds of high heat-conducting powder fillers with different particle size ranges and one or two kinds of matched silane coupling agents. Through the collocation and the processing of filler for the addition of filler increases, thereby accomplishes the purpose that promotes coefficient of heat conductivity, for the constantly growing application of heat dissipation capacity provides the heat dissipation scheme, for the chip protection driving that calorific capacity constantly increases.
Specifically, the first aspect of the present invention provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the content of the micron-sized inorganic filler is at least not lower than 55 wt% of the high thermal conductivity interface material.
As a preferred technical solution of the present invention, the micron-sized inorganic filler at least comprises micron-sized aluminum nitride and micron-sized aluminum oxide; the content of the micron-grade aluminum oxide is not lower than that of the micron-grade aluminum nitride.
In a preferred embodiment of the present invention, the micron-sized alumina includes spherical alumina particles and amorphous alumina particles.
As a preferable technical scheme of the invention, the content ratio of the spherical alumina particles to the amorphous alumina particles is (4-8): (3-8).
In a preferred embodiment of the present invention, the spherical alumina fine particles have a particle size of not more than 15 μm.
As a preferable technical scheme of the invention, the particle size of the spherical alumina particles is not less than 3 microns
In a preferred embodiment of the present invention, the size of the amorphous alumina fine particles is not greater than 1 μm.
As a preferable technical scheme of the invention, the particle size of the micron-sized aluminum nitride is 80-100 microns.
A second aspect of the present invention provides a method for preparing the high thermal conductivity interface material, which comprises the following steps:
(1) adding the binding material into a stirrer, stirring and mixing, then adding the micron-sized inorganic filler in batches, and stirring and mixing under a vacuum condition;
(2) and respectively adding a polymerization inhibitor and a catalyst into the system in sequence, and stirring and mixing under a vacuum condition to obtain the catalyst.
As a preferred technical solution of the present invention, the step (1) of adding the micron-sized inorganic filler in batches includes the following steps:
1) adding amorphous alumina particles with required weight into a stirrer, and stirring for 20-40min under a vacuum condition;
2) adding spherical alumina particles with required weight into the system, and stirring for 5-15min under vacuum condition;
3) dividing micron-sized aluminum nitride into 3 parts by equal weight, adding the first part of micron-sized aluminum nitride into the system, and stirring for 5-15min under a vacuum condition; then adding a second part of the micron-sized aluminum nitride, and stirring for 5-15min under a vacuum condition; and then adding a third part of the micron-sized aluminum nitride, and stirring for 5-15min under a vacuum condition to finish the batch addition of the micron-sized inorganic filler.
Has the advantages that: the thermal conductivity of the heat conduction material is in direct proportion to the addition of the filler, but the filler cannot be added after being added to a certain amount, and the limit of the thermal conductivity can only be about 5W/m-K. The invention adopts the aluminum nitride filler with higher heat conduction number as the heat conduction framework, the alumina micro powder particles fill the gaps to improve the heat conduction coefficient (8-10W/m-K) of the heat conduction material, and the surface of the filler is pretreated by the silane coupling agent, so that the obtained interface material has excellent rheological property and can meet the requirement of an automatic dispensing process, thereby achieving the purpose of improving the heat conduction coefficient, providing a heat dissipation scheme for the application of continuously increasing heat dissipation capacity and protecting the chip with continuously increasing heat productivity.
Detailed Description
The technical features of the technical solutions provided by the present invention will be further clearly and completely described below with reference to the specific embodiments, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
When a parameter is expressed herein as a range, preferred range, or as a range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "0.1 to 1" is disclosed, the described range should be interpreted to include the ranges "0.1 to 0.9", "0.1 to 0.8", "0.1 to 0.7", "0.1 to 0.6 and 0.7 to 1", "0.1 to 0.8 and 1", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The first aspect of the present invention provides a high thermal conductivity interface material, which includes a micron-sized inorganic filler and a binder; the content of the micron-sized inorganic filler is at least not lower than 55 wt% of the high thermal conductivity interface material.
The micron-sized inorganic filler in the binder binding system of the present invention may be any of various thermoplastic elastomers, thermoplastic rubbers, etc. known to those skilled in the art, including but not limited to silicone oil, polyurethane, various natural rubbers, synthetic rubbers, etc.
In some embodiments, the binder silicone oil.
In some preferred embodiments, the silicone oil comprises a vinyl silicone oil and a hydrogen-terminated silicone (Si — H crosslinker).
In some preferred embodiments, the vinyl silicone oil and the terminal hydrogen-containing silicone have the same viscosity; preferably, a silicone oil having a viscosity of about 100cps is used.
In some preferred embodiments, the vinyl silicone oil is present in an amount of 3 to 10wt% based on the total weight of the high thermal interface material.
In some preferred embodiments, the hydrogen-terminated silicone is present in an amount of 0.5 to 3wt% based on the total weight of the high thermal interface material.
According to the invention, the binding material is effectively compounded between vinyl silicone oil with specific viscosity and terminal hydrogen-containing organic silicon (Si-H), so that in the preparation process of the high-thermal-conductivity interface material, under the action of heat or a catalyst and the like, addition reaction between hydrogen on the terminal hydrogen-containing organic silicon and unsaturated double bonds on the vinyl silicone oil is promoted to form a cross-linked network structure, micron-sized inorganic filler in the system is uniformly distributed and fixed in the system, and the interface material with excellent performance is obtained through molding. When the compatibility proportion between the hydrogen-containing silicone and the vinyl silicone oil is not proper or a certain component is lacked, the internal microstructure of the interface material is influenced, and the normal forming and use of the interface material are influenced.
In some embodiments, the binder further comprises a coupling agent.
Preferably, the coupling agent is an organosiloxane coupling agent.
More preferably, the content of the organic siloxane coupling agent is 0.01-0.1 wt%.
The specific components and selection of the organosiloxane coupling agent in the present invention are not particularly limited, and various components known to those skilled in the art may be selected. In some preferred embodiments, the organosiloxane coupling agent is selected from 3-methoxysiloxanes having 10 carbon chains. By adding a certain amount of organic siloxane coupling agent into the bonding material, the applicant finds that the fluidity of the heat-conducting interface material can be effectively improved, so that the heat-conducting interface material has excellent rheological property on the premise of containing a large amount of micron-sized inorganic filler, the interface material can be applied to an automatic dispensing process, and the application range and the use efficiency of the interface material are enlarged.
Certain amounts of catalyst and polymerization inhibitor are also added to the binder of the present invention.
The catalyst in the present invention is not particularly limited, and various catalyst components known to those skilled in the art that can catalyze the addition reaction between vinyl silicone oil and hydrogen-terminated silicone oil can be selected, including but not limited to platinum catalyst. The polymerization inhibitor in the present invention is not particularly limited, and various polymerization inhibitors known to those skilled in the art that can prevent the addition reaction between vinyl silicone oil and hydrogen-terminated silicone oil can be selected, including but not limited to hydroquinone methyl ether, etc.
The micron-sized inorganic filler is an inorganic filler component with the average particle size or the size of 0.1-1000 microns, wherein the specific micro/macro morphology of the micron-sized inorganic filler is not specially limited, and various inorganic fillers can be adopted, including but not limited to nearly spherical, elliptical, snowflake, cubic, sheet and the like. The specific components of the inorganic filler in the present invention are not particularly limited, and various inorganic filler components known to those skilled in the art may be selected, including but not limited to various metal oxides, metal nitrides, and the like, such as aluminum oxide, aluminum nitride, magnesium oxide, copper oxide, iron oxide, and the like.
The content of the micron-sized inorganic filler in the invention is not less than 55 wt%; preferably, the content of the micron-sized inorganic filler is not less than 65 wt%; preferably, the content of the micron-sized inorganic filler is not less than 75 wt%; further preferably, the content of the micro-sized inorganic filler is not less than 85 wt%.
In some embodiments, the micron-sized inorganic filler comprises at least micron-sized aluminum nitride and micron-sized aluminum oxide; the content of the micron-grade aluminum oxide is not lower than that of the micron-grade aluminum nitride. Because micron-sized inorganic filler in the system needs to be bonded and molded by the binder, the binder needs to ensure a certain content, and the content of the inorganic filler in the binder cannot be too high, which directly affects the heat-conducting performance of the heat-conducting interface material. The micron-sized aluminum nitride adopted in the application has better heat-conducting property, and the heat-conducting coefficient is more than five times that of micron-sized aluminum oxide. The applicant finds that the micron-sized aluminum nitride component with higher heat conductivity coefficient is used as the heat conducting framework of the heat conducting interface material, and a proper amount of micron-sized alumina particles are filled in gaps formed by the aluminum nitride heat conducting framework, so that the heat conducting performance of the interface material can be remarkably improved, and the heat conductivity coefficient of the interface material is increased to 8-10W/m-K from the conventional interface material which is lower than about 5W/m-K. Wherein, because the micron-sized aluminum nitride plays a role of a heat conducting framework in the interface material, the dosage of the micron-sized aluminum nitride is higher than that of the micron-sized aluminum oxide, and the micron-sized aluminum nitride can play a role of full support.
In some embodiments, the micron-sized alumina comprises spherical alumina particles and amorphous alumina particles; preferably, the content ratio of the spherical alumina particles to the amorphous alumina particles is (4-8): (3-8); preferably, the content of the spherical alumina particles and the amorphous alumina particles in the heat conducting interface material is 20-40 wt% and 5-40 wt%, respectively.
In some preferred embodiments, the spherical alumina particulates have a particle size of no greater than 15 microns.
In some preferred embodiments, the spherical alumina particulates have a particle size of not less than 3 microns.
More preferably, the spherical alumina fine particles have a particle diameter of 3 to 10 μm.
More preferably, the spherical alumina fine particles have a particle diameter of 6 to 7 μm
The particle size of the fine particles in the present invention refers to an average particle size, and can be measured by methods known to those skilled in the art, such as scanning electron microscopy, X-ray diffraction, and the like.
In some preferred embodiments, the amorphous alumina particulates are no greater than 1 micron in size; preferably, the size of the amorphous alumina particles is not less than 0.1 micron; preferably, the size of the amorphous alumina particles is 0.1-1 micron; more preferably, the size of the amorphous alumina fine particles is 0.4 to 0.6 μm. The size of the amorphous alumina fine particles in the present invention refers to the largest size among three-dimensional sizes of the fine particles.
In some embodiments, the micron-sized aluminum nitride has a particle size greater than the particle size/dimension of the micron-sized alumina.
In some preferred embodiments, the micron-sized aluminum nitride has a particle size of not less than 60 microns; preferably, the particle size is not less than 80 microns; preferably, the particle size is not higher than 120 μm.
In some preferred embodiments, the micron-sized aluminum nitride has a particle size of 80 to 100 microns.
In the process of completing the invention, the applicant finds that the heat-conducting property of the interface material can be improved to a great extent by compounding micron-sized aluminum oxide with different particle sizes and micron-sized aluminum nitride. Through the aluminum nitride with larger grain diameter, a continuous, stable and evenly distributed heat conduction framework is formed in the interface material, and the heat received by the system is rapidly transferred. And because the gap size that the skeleton formed can not guarantee evenly, consequently form the gap of various sizes in the system, through the regulation and control to micron level alumina size, make it fully to fill the gap that the skeleton material formed, avoid because the heat transfer that the gap caused is not smooth, influence the promotion of coefficient of heat conductivity. The applicant finds that when the grain size of micron-sized aluminum nitride is 80-100 microns, and the aluminum oxide adopts two specifications of aluminum oxide components with the grain sizes of 3-10 microns and 0.1-1 micron, the microstructure of the obtained interface material is sufficiently compact and uniform, the heat transfer capacity is optimal, and therefore the heat conductivity coefficient of the interface material is remarkably improved.
A second aspect of the present invention provides a method for preparing the high thermal conductivity interface material, which comprises the following steps:
(1) adding the binding material into a stirrer, stirring and mixing, then adding the micron-sized inorganic filler in batches, and stirring and mixing under a vacuum condition;
(2) and respectively adding a polymerization inhibitor and a catalyst into the system in sequence, and stirring and mixing under a vacuum condition to obtain the catalyst.
In some preferred embodiments, the batch addition of the micron-sized inorganic filler in step (1) comprises the steps of:
1) adding amorphous alumina particles with required weight into a stirrer, and stirring for 20-40min under a vacuum condition;
2) adding spherical alumina particles with required weight into the system, and stirring for 5-15min under vacuum condition;
3) dividing micron-sized aluminum nitride into 3 parts by equal weight, adding the first part of micron-sized aluminum nitride into the system, and stirring for 5-15min under a vacuum condition; then adding a second part of the micron-sized aluminum nitride, and stirring for 5-15min under a vacuum condition; and then adding a third part of the micron-sized aluminum nitride, and stirring for 5-15min under a vacuum condition to finish the batch addition of the micron-sized inorganic filler.
In some preferred embodiments, the method for preparing the interface material with high thermal conductivity comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding 0.1-1 micron alumina, and stirring for 30 minutes at the rotating speed of 30rpm under the vacuum condition;
3) adding 3-10 micron alumina, and stirring at 30rpm under vacuum condition for 10 min;
4) adding 8-100 micron aluminum nitride (1/3), stirring at 30rpm under vacuum for 10 min;
5) adding 8-100 micron aluminum nitride (2/3), stirring at 30rpm under vacuum for 10 min;
6) adding 8-100 micron aluminum nitride (3/3), stirring at 30rpm under vacuum for 10 min;
7) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
8) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
9) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
The applicant finds that the adding sequence of materials in the process of preparing the high-thermal-conductivity interface material is very critical, and the relation of the quality of the thermal conductivity of the interface material is written in a Chinese character mi. When the amorphous alumina with the minimum size is added into the binder, the amorphous alumina is blended under a vacuum condition, then the spherical micron-grade alumina with the size of 3-10 microns is added, the mixture is blended, and the rest of the aluminum nitride is added in batches, the obtained interface material has the best thermal conductivity, and the excellent rheological property and the glue yield can be ensured, so that the interface material has a more excellent use process and a wider application environment.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
Examples
Example 1: the embodiment provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the micron-sized inorganic filler is present in an amount of about 95.5 wt% of the high thermal conductivity interface material.
The high-thermal-conductivity interface material is prepared from the following raw materials:
the average grain diameter of the micron-sized aluminum nitride is 70 microns; the particle size of the spherical alumina (3-10 micron alumina) is 6 microns; the amorphous alumina (0.1-1 micron alumina) has an average size of 0.5 micron; the silane coupling agent is N-N-butyl-3-aminopropyltrimethoxysilane; the polymerization inhibitor is hydroquinone methyl ether; the terminal hydrogen-containing organic silicon is 100cps hydrogen-containing silicone oil of Shandong Dayi chemical industry Co.
The preparation method of the high-thermal-conductivity interface material comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding amorphous alumina, and stirring for 30 minutes under vacuum at the rotating speed of 30 rpm;
3) adding spherical alumina, and stirring at 30rpm under vacuum for 10 minutes;
4) micron-sized aluminum nitride (1/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
5) micron-sized aluminum nitride (2/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
6) micron-sized aluminum nitride (3/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
7) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
8) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
9) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
Example 2: the embodiment provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the micron-sized inorganic filler is present in an amount of about 94 wt% of the high thermal conductivity interface material.
The high-thermal-conductivity interface material is prepared from the following raw materials:
the average grain diameter of the micron-sized aluminum nitride is 70 microns; the particle size of the spherical alumina (3-10 micron alumina) is 6 microns; the amorphous alumina (0.1-1 micron alumina) has an average size of 0.5 micron; the silane coupling agent is N-N-butyl-3-aminopropyltrimethoxysilane; the polymerization inhibitor is hydroquinone methyl ether; the terminal hydrogen-containing organic silicon is 100cps hydrogen-containing silicone oil of Shandong Dayi chemical industry Co.
The preparation method of the high-thermal-conductivity interface material comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding amorphous alumina, and stirring for 30 minutes under vacuum at the rotating speed of 30 rpm;
3) adding spherical alumina, and stirring at 30rpm under vacuum for 10 minutes;
4) micron-sized aluminum nitride (1/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
5) micron-sized aluminum nitride (2/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
6) micron-sized aluminum nitride (3/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
7) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
8) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
9) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
Example 3: the embodiment provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the content of the micron-sized inorganic filler accounts for the high heat-conducting interfaceAbout 95.5 wt% of the material.
The high-thermal-conductivity interface material is prepared from the following raw materials:
the average grain diameter of the micron-sized aluminum nitride is 70 microns; the particle size of the spherical alumina is 6 microns; the silane coupling agent is N-N-butyl-3-aminopropyltrimethoxysilane; the polymerization inhibitor is hydroquinone methyl ether; the terminal hydrogen-containing organic silicon is 100cps hydrogen-containing silicone oil of Shandong Dayi chemical industry Co.
The preparation method of the high-thermal-conductivity interface material comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding spherical alumina, and stirring at 30rpm under vacuum for 10 minutes;
3) micron-sized aluminum nitride (1/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
4) micron-sized aluminum nitride (2/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
5) micron-sized aluminum nitride (3/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
6) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
7) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
8) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
Example 4: the embodiment provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the micron-sized inorganic filler is present in an amount of about 95.5 wt% of the high thermal conductivity interface material.
The high-thermal-conductivity interface material is prepared from the following raw materials:
the average grain diameter of the micron-sized aluminum nitride is 70 microns; the amorphous alumina (0.1-1 micron alumina) has an average size of 0.5 micron; the silane coupling agent is N-N-butyl-3-aminopropyltrimethoxysilane; the polymerization inhibitor is hydroquinone methyl ether; the terminal hydrogen-containing organic silicon is 100cps hydrogen-containing silicone oil of Shandong Dayi chemical industry Co.
The preparation method of the high-thermal-conductivity interface material comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding amorphous alumina, and stirring for 30 minutes under vacuum at the rotating speed of 30 rpm;
3) micron-sized aluminum nitride (1/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
4) micron-sized aluminum nitride (2/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
5) micron-sized aluminum nitride (3/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
6) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
7) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
8) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
Example 5: the embodiment provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the micron-sized inorganicThe filler content is about 95.5 wt% of the high thermal conductivity interface material.
The high-thermal-conductivity interface material is prepared from the following raw materials:
the average grain diameter of the micron-sized aluminum nitride is 100 microns; the particle size of the spherical alumina (3-10 micron alumina) is 6 microns; the amorphous alumina (0.1-1 micron alumina) has an average size of 0.5 micron; the silane coupling agent is N-N-butyl-3-aminopropyltrimethoxysilane; the polymerization inhibitor is hydroquinone methyl ether; the terminal hydrogen-containing organic silicon is 100cps hydrogen-containing silicone oil of Shandong Dayi chemical industry Co.
The preparation method of the high-thermal-conductivity interface material comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding amorphous alumina, and stirring for 30 minutes under vacuum at the rotating speed of 30 rpm;
3) adding spherical alumina, and stirring at 30rpm under vacuum for 10 minutes;
4) micron-sized aluminum nitride (1/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
5) micron-sized aluminum nitride (2/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
6) micron-sized aluminum nitride (3/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
7) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
8) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
9) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
Example 6: the embodiment provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the micron-sized inorganic filler is present in an amount of about 95.5 wt% of the high thermal conductivity interface material.
The high-thermal-conductivity interface material is prepared from the following raw materials:
the average grain diameter of the micron-sized aluminum nitride is 70 microns; the average size of the spherical alumina (3-10 micron alumina) and the amorphous alumina (0.1-1 micron alumina) is 20 microns; the silane coupling agent is N-N-butyl-3-aminopropyltrimethoxysilane; the polymerization inhibitor is hydroquinone methyl ether; the terminal hydrogen-containing organic silicon is 100cps hydrogen-containing silicone oil of Shandong Dayi chemical industry Co.
The preparation method of the high-thermal-conductivity interface material comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding amorphous alumina, and stirring for 30 minutes under vacuum at the rotating speed of 30 rpm;
3) adding spherical alumina, and stirring at 30rpm under vacuum for 10 minutes;
4) micron-sized aluminum nitride (1/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
5) micron-sized aluminum nitride (2/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
6) micron-sized aluminum nitride (3/3) is added and stirred for 10 minutes under vacuum condition at the rotating speed of 30 rpm;
7) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
8) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
9) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
Example 7: the embodiment provides a high thermal conductivity interface material, which comprises a micron-sized inorganic filler and a binder; the micron-sized inorganic filler is present in an amount of about 95.5 wt% of the high thermal conductivity interface material.
The high-thermal-conductivity interface material is prepared from the following raw materials:
the average grain diameter of the micron-sized aluminum nitride is 70 microns; the particle size of the spherical alumina (3-10 micron alumina) is 6 microns; the amorphous alumina (0.1-1 micron alumina) has an average size of 0.5 micron; the silane coupling agent is N-N-butyl-3-aminopropyltrimethoxysilane; the polymerization inhibitor is hydroquinone methyl ether; the terminal hydrogen-containing organic silicon is 100cps hydrogen-containing silicone oil of Shandong Dayi chemical industry Co.
The preparation method of the high-thermal-conductivity interface material comprises the following steps:
1) adding vinyl silicone oil, a Si-H cross-linking agent (hydrogen-containing silicone at the end) and a silane coupling agent into a double-planet stirrer, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
2) adding amorphous alumina, and stirring for 30 minutes under vacuum at the rotating speed of 30 rpm;
3) adding spherical alumina, and stirring at 30rpm under vacuum for 10 minutes;
4) adding micron-sized aluminum nitride, and stirring for 10 minutes at the rotating speed of 30rpm under the vacuum condition;
5) adding a polymerization inhibitor, and stirring for 10 minutes at the rotating speed of 30rpm under a vacuum condition;
6) adding a platinum catalyst, and stirring for five minutes under a vacuum condition at the rotating speed of 30 rpm;
7) and (3) filling the completely stirred materials into a rubber tube with a certain volume, and storing the rubber tube in a room temperature environment for later use.
Performance testing
The applicant carries out the heat conductivity coefficient, viscosity and glue yield tests on the interface material samples in the above embodiments, and the specific test method comprises the following steps:
(1) and (3) testing the heat conductivity coefficient: the thermal conductivity was measured using the test standard of ASTM D5470, and the results are shown in table 1 below.
(2) And (3) viscosity testing: the viscosity test was carried out using a rheometer DHR-2 from TA, 0 degree rotor, at a shear rate of 11/s, and the results are shown in Table 1 below.
(3) Testing the glue yield: the glue output is measured by an EFD semi-automatic dispenser, the glue is filled in a 10cc EDF rubber tube, the glue is squeezed out by 90psi pressure, the glue output within 1 minute is measured, and the measurement results are shown in the following table 1.
Table 1 results of performance testing
| Coefficient of thermal conductivity (W/m-K) | viscosity/(Pa.s) | Glue yield/(g/min) | |
| Example 1 | 8.9 | 1088 | 15.2 |
| Example 2 | 5.5 | 1550 | 20.1 |
| Example 3 | 6.3 | 1291 | 10.2 |
| Example 4 | 6.1 | 1202 | 5.3 |
| Example 5 | 8.1 | 1710 | 20.8 |
| Example 6 | 7.2 | 1468 | 12.0 |
| Example 7 | 3.4 | >2000 | --- |
From the experimental results, the aluminum nitride filler with higher heat conduction number is used as the heat conduction framework, the gaps are filled with the alumina micro powder particles to improve the heat conduction coefficient of the heat conduction material, and the surface of the filler is pretreated by the silane coupling agent, so that the mixed material has excellent rheological property and can meet the requirement of an automatic dispensing process.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content disclosed above into an equivalent embodiment with equivalent changes, but all those simple modifications, equivalent changes and modifications made on the above embodiment according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (2)
1. The high heat conducting interface material is characterized by comprising micron-sized inorganic filler and a binding material; the content of the micron-sized inorganic filler is at least not lower than 55 wt% of the high thermal conductivity interface material;
the bonding material is organic silicone oil, and the organic silicone oil comprises vinyl silicone oil and hydrogen-terminated organic silicon;
the content of the vinyl silicone oil accounts for 3-10wt% of the total weight of the high thermal conductivity interface material, and the content of the hydrogen-terminated silicone oil accounts for 0.5-3wt% of the total weight of the high thermal conductivity interface material;
the micron-sized inorganic filler at least comprises micron-sized aluminum nitride and micron-sized aluminum oxide; the content of the micron-grade aluminum oxide is not lower than that of the micron-grade aluminum nitride;
the micron-scale alumina comprises spherical alumina particles and amorphous alumina particles;
the particle size of the spherical alumina particles is not higher than 15 microns, and the particle size is not lower than 3 microns;
the size of the amorphous alumina particles is not higher than 1 micron;
the grain size of the micron-sized aluminum nitride is 80-100 microns;
the high-thermal-conductivity interface material is prepared by the following preparation method:
(1) adding the binding material into a stirrer, stirring and mixing, then adding the micron-sized inorganic filler in batches, and stirring and mixing under a vacuum condition;
(2) respectively adding a polymerization inhibitor and a catalyst into the system in sequence, and stirring and mixing under a vacuum condition to obtain the catalyst;
the batch adding mode of the micron-sized inorganic filler in the step (1) of the preparation method comprises the following steps:
1) adding amorphous alumina particles with required weight into a stirrer, and stirring for 20-40min under a vacuum condition;
2) adding spherical alumina particles with required weight into the system, and stirring for 5-15min under vacuum condition;
3) dividing micron-sized aluminum nitride into 3 parts by equal weight, adding the first part of micron-sized aluminum nitride into the system, and stirring for 5-15min under a vacuum condition; then adding a second part of the micron-sized aluminum nitride, and stirring for 5-15min under a vacuum condition; and then adding a third part of the micron-sized aluminum nitride, and stirring for 5-15min under a vacuum condition to finish the batch addition of the micron-sized inorganic filler.
2. The high thermal interface material as claimed in claim 1, wherein the ratio of the spherical alumina particles to the amorphous alumina particles is (4-8): (3-8).
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| CN109749408A (en) * | 2018-12-25 | 2019-05-14 | 苏州赛伍应用技术股份有限公司 | A kind of heat-conducting interface material and its preparation method and application |
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| CN109749408A (en) * | 2018-12-25 | 2019-05-14 | 苏州赛伍应用技术股份有限公司 | A kind of heat-conducting interface material and its preparation method and application |
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